safrole isomerization without reflux ???

[methlab]

Hi guys! I did not want to buy again this expensive PdCl2, that's why i thought i should follow the performic. To learn i started to isomerize 50g pure Safrole. I added KOH and warmed up to remove water first, solution turned dark brown. After removing water i wanted to start reflux, but than i got an important phonecall and i had to leave the house, sealed the cooled 250ml rbf and left. After about 1 1/2 days i wanted to continue the reaction, but the mix did not start to boil at about 225 C, as it normally does! It started to boil at about 244-248 C ! This is the bp for iso here (see chromic's bp table for safrole and isosafrole). Could this be true ? Has the Safrole converted to iso just without reflux ? Greetings

[ApprenticeCook]

whack the crap in a vacuum distillation set, heat it up to iso bp and see what happens, if it has tell the hive, bee most usefull if it did happen but over 1.5 days not on reflux compared to an overnight job running the reflux? include yields and comments to see if that made it better/worse.

[methlab]

when heating up i recognized that there is still safrole in it, so i did a vacuum reflux over night, to convert the rest. I don't know how much has been converted before the vacuum reflux, but it seem to be useless. The only thing that was interessting for me was, that the vacuum is much stronger (about +50%) since i am using a vacuum-hose instead of a normal PE hose, which sqeezed a little bit after applying the vacuum.